Mesoporous materials type TiMCM41 prepared by hydrothermal and ultrasoundassisted techniques were characterized by XRD, SEM, TEM, nitrogen physisorption, ammonia TPD, UVvis and FTIR. Both showed the MCM41 characteristic structure. Hydrothermal treatment allowed obtaining a well ordered material and ultrasound procedure gave a better titanium distribution. Electronic microscopy images revealed Ti dispersion zones as well as the quantity of metal in the structure. The catalytic activity of these materials were tested by acetylation of aromatic and steroidal alcohols to afford the corresponding esters in good yields.